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Dimethylformamide → Sulfo(2,3-dihydro-5-benzofuranyl)acetyl chloride

HRID 1390218
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HRID 1390218 반응식
[S:1]([CH:5]([C:9]1[CH:10]=[CH:11][C:12]2[O:16][CH2:15][CH2:14][C:13]=2[CH:17]=1)[C:6](O)=[O:7])([OH:4])(=[O:3])=[O:2].S(Cl)([Cl:20])=O.CN(C)C=O>CCOCC.CCCCCC>[S:1]([CH:5]([C:9]1[CH:10]=[CH:11][C:12]2[O:16][CH2:15][CH2:14][C:13]=2[CH:17]=1)[C:6]([Cl:20])=[O:7])([OH:4])(=[O:3])=[O:2]
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참가 물질

6

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 23335828Sulfo(2,3-dihydro-5-benzofuranyl)acetic acid

생성물 1

HCID 23335837Sulfo(2,3-dihydro-5-benzofuranyl)acetyl chloride

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8058Hexane용매

실험 절차

Sulfo(2,3-dihydro-5-benzofuranyl)acetyl chloride is prepared according to the general procedure described in J. Med. Chem., 15, 1105 (1972). Sulfo(2,3-dihydro-5-benzofuranyl)acetic acid (20 mmole) is added slowly to a solution of ether (4 ml) and thionyl chloride (150 mmole). The mixture is stirred at room temperature until the gas evolution stopped. Then about 0.2 ml of dimethylformamide is added and the solution heated at 40° C. for 4 hours. The mixture is diluted with 30 ml of ether and 30 ml of hexane and then cooled to -25° C. Sulfo(2,3-dihydro-5-benzofuranyl)acetyl chloride is recovered from the mixture and used without further purification.

후처리

  1. temperaturethe solution heated at 40° C. for 4 hours
  2. temperaturecooled to -25° C
  3. customSulfo(2,3-dihydro-5-benzofuranyl)acetyl chloride is recovered from the mixture
  4. customused without further purification

출처 및 근거

ORD 기록
ord-6ece8161c25f42f381ae84e7369f6b79
출처 데이터셋
uspto-grants-1979_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04138397

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